RESUMO
An accurate and reliable HPLC-MS/MS method has been established for the simultaneous determination of seven toxic components in the Chinese medicine ShenFuTuoDu capsules. The seven toxic components were separated on a Shimadzu Shim-pack GIST C18 column (3.0 mm×50 mm, 3.0 µm) with methanol and water (containing 0.1% formic acid) as the mobile phase by gradient elution. The flow rate was 0.5 mLâ¢min-1. The column temperature was 25°C and the injection volume was 5µL. An ESI+ scan combined with MRM was adopted and the instrument parameters were as follows: ion source voltage, 5.5 kV; ion source temperature, 600oC; curtain gas, 68.95 kPa; atomized gas, 344.75 kPa; auxiliary gas, 344.75 kPa. The linear relationships of the seven components were good (R2>0.9937). The average recoveries were 95.2%-106.7% with RSD of 0.79%-5.27% (n=6). The seven toxic components of scopolamine, atropine, rhynchophylline, isorhynchophylline, benzoylaconine, benzoylmesaconine and benzoylhypaconine in six batches of ShenFuTuoDu capsules were 5.99-18.48µgâ¢g-1, 6.36-14.79µgâ¢g-1, 3.71-15.45µgâ¢g-1, 7.90-15.08µgâ¢g-1, 19.05-44.58µgâ¢g-1, 117.38-248.26µgâ¢g-1 and 19.74-79.49µgâ¢g-1, respectively. Precision, stability and repeatability test RSDs were less than 7.17% (n=6). The method is suitable for the simultaneous determination of scopolamine, atropine, rhynchophylline, isorhynchophylline, benzoylaconine, benzoylmesaconine and benzoylhypaconine. It can be used for the quality control of ShenFuTuoDu capsules.
